Preparation of adsorbents



Patented Aug. 11, 1931 I UNITED STATES PATENT OFFICE ROY CROSS, OFKANSAS CITY, MISSOURI, ASSIGNOR '10 CROSS DEVELOPMENT CORPORA- TION, ACORPORATION OF DELAWARE PREPARATION OF .ADSORBENTS No Drawing. Originalapplication filed December 22, 1921, Serial No. 524,290. Divided andthis application filed November 10, 1923. Serial No 674,043.

This application is a divisional of an original application, SerialNo.524,290, filed under date of December 22nd, 1921.

My invention relates to a method of treating hydrocarbons and has forits object the dehydration, decolorization and neutralization of oil'bythe intimate contacting of theoil either in the liquid or vapor statewith dried hydrous silicate of alumina. The most valuable hydroussilicate of alumina or Zeolite for this purpose is the-- naturallyoccurring substance known as Bentonite. Bentonite is the best of thisclass of adsorbent material and is possibly the active principle to befound in fullers earth. A typical quality of Bentonite is that. foundnear Ardmore, South Dakota, and has the following composition:

This material has the property of absorb ing a very large amount ofwater, forming a gelatinous mass with it and is capable of being dilutedwith water and forming a colloid to such a degree that the waterpermanently remains milky.

For the purpose of use, the hydrous silicate of alumina is perfectlydried but not ignited. It is then crushed and screened to the sizesdesired. For some purposes it is used in a finely divided powder, othersas coarse granules. For the dehydration of oils, the coarse granules arebest as they absorb the water from the oil without producing aturbidity. For decolorizing lubricating oils, the coarse granules arebest as they form a bed more pervious to the passage of the oil. Toobtain the greatest de-v colorizing action, however, the more finely,

passing dry chlorine over the hot hydrous silicate of alumina. Thisrenews the absorptive effect of the hydrous silicate of alumina and inaddition, forms a small amount of anhydrous aluminum chloride, becauseof the chemical susceptibility of the aluminum silicate in this form.

When rejuvenated by chlorine, however, the hydrous silicate of aluminamust be kept in perfectly dry.containers.-

The method of applying the hydrous silicate of alumina to the oildepends upon the character of the oil to be treated. In the case ofpressure benzine or gasoline such as is obtained in the ordinarycracking plant, the color of the gasoline is such that it cannot bemarketed under the ordinar Navy specifications. Decolorization is efected by pumping the gasoline through a warm bed of hydrous silicate ofalumina and discharging ,it into a still containing hydrous silicate ofalumina. The vapors arising from the still are made to pass and theamount of hydrous silicate of alumina required varies with the characterof the distillate. Ordinarily when rocesses such as the Cross process,described in Patent No. 1,423,500, are used, one pound of hydroussilicate of alumina in finely divided condition is suflicient for onepound of gasoline.

If the hydrous silicate of alumina is placed in the still ,alone alarger quantity is required. When distillation is complete, the

hydrous silicate of alumina is steamed out to remove all of the oil andthe particles have a greenish to black appearance. The used hydroussilicate of alumina is now placed in the ordinary fullers earth burners-'in which the volatile carbonaceous matter is removed. From the fullersearth burner it is discharged into a vertical tile tower through whichis passed a current of dry chlorine gas at such a rate and in suchquantity that the chlorine gas does not appreciably escape from the top.The residue at the bottom'is drawn OE and again used. When the residueafter treatment with chlorine is used, it has been found that thegasoline distilled has a' lower end point and a lower content of olefincompounds and the odor of the gasoline is considerably improved.

In the dehydration of petroleum, the petroleum only has to pass throughthe granular hydrous silicate of alumina toremove the water. In thiscase, the hydrous silicate of alumina is regenerated merely by heatingto drive off the moisture until it becomes so impregnated withcarbonaceous matter that it issubjected to the treatment hereindescribed for revivifying the exhausted material.

ing the material, and subjecting the treated material to the action ofdry chlorine gas, as and for the purpose described.

5. A process for revivifying and modifying the character of spentbentonite resulting from the treatment of oils with bentonite, whichcomprises driving ofl:' adsorbedv volatile carbonaceous substancesretained in the spent bentonite, and thereafter treating the bentonitewith chlorine gas.

ROY GRUSS.

In the treatment of kerosene or other refined petroleum, which haspreviously been treated with acid, the hydrous silicate of aluminaremoves the last trace of acid as well as decolorizes and dehydrates theoil.

The treatment of lubricants with hydrous silicate of alumina isaccomplished in the same manner as with ordinary fullers earth usingpreferably 20. to 30 mesh material. 'Ihe residual hydrous silicate ofalumina is regenerated in the usual manner except that the added step oftreatment with dry chlorine is used.

For the treatment of transformer oils, hydrous silicate of alumina isparticularly valuable as it removes the last trace of moisture withoutadding anything to the oil which will have a greater conductivity thanthe water even in case thelast traces of hydrous silicate of alumina arenot removed.

I claim as my invention:

1. A process for the revivification and treatment of'bentonite for usein refining 011, comprising passing dry chlorine; gas in contacttherewith at temperatures sufficiently high to effect a combination ofthe chlorine and alumina constituents.

2. A process for the revivification and treatment of bentonite for usein oil refining, comprising the steps of initially heatmg the material,and passing dry chlorine gas thereover sufiiciently heated to efiect acombination of the chlorine and alumina constitutents. p

3. A process for the revivification and treatment of bentonite,comprising initially

